A kind of synthetic method of efficient polymerization inhibitor 701
A synthesis process, the technology of nitroxide free radical piperidinol, which is applied in the field of synthesis process of 701, can solve the problems of complex equipment and excessive energy consumption, meet the requirements of simplifying equipment and process, reduce energy consumption, and reduce the cost of equipment The effect of corrosion
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Embodiment 1
[0057] 120g of tetramethylpiperidinol, 35g of water, 0.8g of magnesium hydroxide and 0.12g of sodium bicarbonate were added to the reaction flask;
[0058] Under stirring, slowly add 30 (weight)% hydrogen peroxide dropwise, maintain the temperature in the reaction flask at 50~55 ℃, after the dropwise addition of hydrogen peroxide is completed, continue to heat the reaction at 50~55 ℃;
[0059] After the reaction, add 0.5 g of manganese dioxide to destroy excess hydrogen peroxide;
[0060] Filtration, the obtained filtrate is carried out low pressure distillation, and the solid is sliced after the distillation finishes to obtain product 701 (nitroxide radical piperidinol), and the yield is 98.5%, which is an orange-yellow crystal, and GC chromatography detects that its purity is about 99.5%, Its GC chromatogram is as follows figure 1 As shown, it can be seen that there are peak positions at the residence time (min.) of 1.572, 4.658, 5.598, 6.531, 7.129, 21.019 and 21.627, wh...
Embodiment 2
[0062] 100g of tetramethylpiperidinol, 30g of water, 0.7g of magnesium hydroxide and 0.1g of sodium bicarbonate were added to the reaction flask;
[0063] Under stirring, slowly add 30 (weight)% hydrogen peroxide dropwise, maintain the temperature in the reaction flask at 50~55 ℃, after the dropwise addition of hydrogen peroxide is completed, continue to heat the reaction at 50~55 ℃;
[0064] After the reaction, add 0.4 g of manganese dioxide to destroy excess hydrogen peroxide;
[0065] Filtration, the obtained filtrate is subjected to low-pressure distillation, and the solid is sliced after the distillation to obtain product 701 (nitroxide radical piperidinol), the yield is 98.3%, and it is orange-yellow crystals, and its purity is about 99.4% detected by GC chromatography.
Embodiment 3
[0067] 120g of tetramethylpiperidinol, 35g of water, 0.8g of sodium tungstate and 0.12g of sodium EDTA were added to the reaction flask;
[0068] Slowly add 30 (weight)% hydrogen peroxide, maintain the temperature in the reaction flask at 50 to 55°C, and after the dropwise addition of hydrogen peroxide is completed, continue to heat the reaction at 50 to 55°C;
[0069] After the reaction, add 0.5 gram of sodium sulfite to destroy excess hydrogen peroxide;
[0070] Filtration, the obtained filtrate is subjected to low pressure distillation, and the solid is sliced after the distillation to obtain product 701 (nitroxide radical piperidinol), and the yield is 98.1%, which is an orange mixed crystal powder, and its purity detected by GC chromatography is about 99.3 %.
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